CN111100750A - Waste fluoride oil treatment method and system - Google Patents

Waste fluoride oil treatment method and system Download PDF

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Publication number
CN111100750A
CN111100750A CN201811266447.8A CN201811266447A CN111100750A CN 111100750 A CN111100750 A CN 111100750A CN 201811266447 A CN201811266447 A CN 201811266447A CN 111100750 A CN111100750 A CN 111100750A
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oil
filtering
waste
reaction
fluorine
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张耿榕
楼仲洲
李振旭
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Taiwan Environment Scientific Co ltd
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Taiwan Environment Scientific Co ltd
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Priority to CN201811266447.8A priority Critical patent/CN111100750A/en
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M175/00Working-up used lubricants to recover useful products ; Cleaning
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M175/00Working-up used lubricants to recover useful products ; Cleaning
    • C10M175/0016Working-up used lubricants to recover useful products ; Cleaning with the use of chemical agents

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The invention provides a method and a system for treating waste fluorine-containing oil, which remove impurities in the waste fluorine-containing oil through a physical reaction by a plurality of procedures of filtering and physical and chemical reactions, and then add a medicament to react with the waste fluorine-containing oil under a certain temperature range to promote the waste fluorine-containing oil to be recovered to regenerated fluorine-containing oil with the original pH value and visibility, thereby improving the reusability of the waste fluorine-containing oil, being capable of being utilized by industries, improving the production benefit and further achieving the purposes of reducing the cost, reducing the pollution and protecting the environment.

Description

Waste fluoride oil treatment method and system
Technical Field
The invention relates to waste fluorine oil, in particular to a method and a system for treating waste fluorine oil.
Background
The fluorine oil is a fluorine LUBRICANT (also called perfluorinated PFPE) FLUORINATED LUBRICATT, is formed by combining three molecules of carbon, fluorine and oxygen, is a very stable substance, and particularly meets the severe requirements of resisting continuous high temperature, high oxidation environment, strong acid and alkali, chemical resistance and solvent resistance. Wherein, the fluorine vegetable oil can resist high temperature of 250 ℃. The properties of the product are smooth, white, generate dust particles and do not pollute the product, so the product is widely applied to semiconductor processing, high-temperature equipment, operation in severe environment and the like.
However, at present, the recycling of waste fluorine-containing oil is less performed in China, and for equipment manufacturers, fluorine-containing oil is an essential consumable, and in the process of processing or operating machinery or machine equipment, the equipment manufacturers will replace brand new fluorine-containing oil, and the discarded fluorine-containing oil becomes waste fluorine-containing oil, wherein fluorine-containing oil is the most expensive group in all lubricating base oil categories, so that the cost of manufacturers is increased by purchasing brand new fluorine-containing oil, and if the project is not solved, the cost required in the operation process in the factory is greatly increased.
Moreover, the eliminated fluorine-containing oil is not properly recycled, and if the waste fluorine-containing oil is treated improperly and is directly discarded, the waste fluorine-containing oil not only can affect human beings, animals and environmental ecology, but also can cause resource waste, and particularly, the waste fluorine-containing oil can still be recycled after being recycled.
Therefore, it is an objective of the present invention to solve the above problems and disadvantages.
Disclosure of Invention
The invention provides a method and a system for treating waste fluorine oil, and mainly aims to recycle the waste fluorine oil, improve the reusability of the waste fluorine oil, further reduce the cost and have environmental protection benefits.
To achieve the above objects, the present invention provides a method for treating waste fluorocarbon oil, which is suitable for matching with waste fluorocarbon oil, comprising:
(A) a primary filtering step: filtering the waste fluorine oil, and removing impurities in the waste fluorine oil through physical reaction treatment of a solid-liquid separation principle;
(B) the reaction steps are as follows: adding decolorizing adsorbent and alkaline agent, and controlling the temperature to above room temperature to allow the filtered waste fluorine-containing oil to generate physical and chemical reaction
(C) And finally, a filtering step: adsorbing suspended matters of the waste fluorine oil after the physical and chemical reaction, and performing physical reaction treatment by using a settling separation principle to form the regenerated fluorine oil.
According to the above method, in a further implementation, the method further comprises:
the decolorizing adsorbent is selected from attapulgite, activated carbon, bentonite, and zeolite.
The alkaline agent is selected from calcium hydroxide, calcium carbonate, magnesium carbonate, and sodium carbonate.
The temperature range above the normal temperature is 110-150 ℃.
The method for treating the waste fluorine-containing oil also comprises a step (D) of secondary filtering, wherein the step (D) of secondary filtering is arranged between the step (B) of reaction and the step (C) of final filtering, and if the waste fluorine-containing oil cannot be in a light-transmitting state after the step (A) of primary filtering, the step (D) of secondary filtering is used for filtering the waste fluorine-containing oil again so as to improve the light transmittance of the waste fluorine-containing oil.
The dosage of decolorizing adsorbent agent is 0.3-0.5g/L, and the dosage of alkaline agent is 0.3-0.5 g/L.
(A) The temperature of the preliminary filtration step and the final filtration step (C) may not exceed 30 ℃.
The number of the first filtering filter cores is four, the first filtering filter core is connected with the oil inlet, the aperture of the first filtering filter core is 5 mu m, and the aperture of the second filtering filter core, the aperture of the fourth filtering filter core and the aperture of the fourth filtering filter core which are sequentially connected are 0.1 mu m.
In addition, the present invention provides a waste fluorine-containing oil treatment system using the waste fluorine-containing oil treatment method, comprising:
the first filtering device comprises an oil inlet, a filtering path flowing through the oil inlet, a plurality of first filtering filter elements positioned on the filtering path, and at least one regeneration temporary storage tank connected with one of the first filtering filter elements, wherein the first filtering filter elements are used for filtering waste fluorine oil impurities flowing through the filtering water path;
the reaction device is connected with the first filtering device and is provided with a reaction tank connected with the at least one regeneration temporary storage tank, and the reaction tank is used for adding a decoloration adsorption medicament and an alkaline medicament to the filtered waste fluorine oil and controlling the temperature to be in a temperature range above the normal temperature so as to enable the filtered waste fluorine oil to generate a physical and chemical reaction;
and the second filtering device is connected with the reaction device, is provided with a second filtering filter element connected with the reaction tank and an oil outlet connected with the second filtering filter element, and the second filtering filter element is used for adsorbing suspended matters of the waste fluorine oil after the physical and chemical reaction so that the waste fluorine oil forms regenerated fluorine oil and is discharged from the oil outlet.
According to the above system, in a further implementation, further comprising:
first filter equipment still contains the air exhaust pump and set up in aforementioned at least one regeneration groove of keeping in with the loss buffer slot between the air exhaust pump, the air exhaust pump is arranged in helping useless fluorine plain oil to flow in every link is filtered, the loss buffer slot is used for preventing useless fluorine plain oil inflow air exhaust pump.
In view of the foregoing, the present invention provides a method and a system for treating waste fluorine-containing oil, which mainly uses a plurality of filtering and physicochemical reactions to remove impurities in the waste fluorine-containing oil through a physical reaction, and then adds a chemical agent to react with a temperature layer controlled to a certain temperature to restore the waste fluorine-containing oil to a regenerated fluorine-containing oil having an original ph and visibility, thereby improving the reusability of the waste fluorine-containing oil and being capable of being utilized by the industry, and improving the production efficiency to achieve the purposes of reducing cost, reducing pollution and protecting environment.
Drawings
FIG. 1 is a flow chart of an embodiment of the present invention.
Fig. 2 is a flow chart of an embodiment of the present invention (two).
FIG. 3 is a diagram of the architecture of an embodiment of the present invention.
Description of the symbols in the drawings:
10 is (A) a preliminary filtration step; 11 is the reaction step (B); 12 is (C) a final filtration step; 13 is (D) a second filtration step; 20 is a first filtering device; 21 is an oil inlet; 22 is a filtering path; 23 is a first filter cartridge; 24 is a regeneration temporary storage tank; 25 is an air pump; 26 is an escape buffer groove; 30 is a reaction device; 31 is a reaction tank; 40 is a second filtering device; 41 is a second filter cartridge; and 42 is an oil outlet.
Detailed Description
The technical solutions of the present invention will be described clearly and completely below, and it should be apparent that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The foregoing and other aspects, features and advantages of the invention will be apparent from the following more particular description of preferred embodiments, as illustrated in the accompanying drawings.
Example 1:
the invention provides a method for treating waste fluorine-containing oil, which is suitable for being matched with the waste fluorine-containing oil, and as shown in figure 1, the method comprises the following steps:
(A) primary filtering step 10: filtering the waste fluorine-containing oil, and removing impurities in the waste fluorine-containing oil through physical reaction treatment of a solid-liquid separation principle, specifically, when the waste fluorine-containing oil enters the preliminary filtering step (A) 10, three to four solid-liquid separation treatments are needed.
(B) A reaction step 11: adding decolorizing adsorbent agent selected from attapulgite, activated carbon, bentonite and zeolite and alkaline agent, and controlling the temperature to be above room temperature to allow the filtered waste fluorine-containing oil to generate physicochemical reaction. The alkaline agent is selected from calcium hydroxide, calcium carbonate, magnesium carbonate, and sodium carbonate. The attapulgite has a unique crystal structure, so that the attapulgite has a plurality of special physical and chemical properties and technological properties, and the main physical and chemical properties and the technological properties are as follows: cation exchangeability, water absorption, adsorption decolorability; the active carbon is mainly prepared by carrying out high-temperature (600-800 ℃) dry distillation on substances such as wood, wood chips, water fruit shells or coal, decomposing the substances to form low-molecular hydrocarbon and porous carbon residues, and activating the low-molecular hydrocarbon and the porous carbon residues by using hot air or water vapor, wherein the surface of the active carbon is provided with a plurality of capillary pores, and the inner surfaces of the capillary pores and the surfaces of particles have adsorption; the bentonite has strong hygroscopicity and expansibility, can adsorb water with volume being 8-15 times of that of the bentonite, and has volume expansion being several times to 30 times; the zeolite is mainly composed of SiO2, Al2O3 and the crystal structure of aluminosilicate composed of alkali metal, alkaline earth metal or rare earth metal, has a higher specific surface area, and is commonly used as a catalyst, a catalyst carrier, an adsorbent and the like. The dosage of the decoloration adsorption medicament is 0.3-0.5g/L, and the dosage of the alkaline medicament is 0.3-0.5 g/L. The temperature range above the normal temperature is 110-150 ℃, when the decolorizing adsorbent agent and the alkaline agent are added, the temperature can not exceed 150 ℃, otherwise, the process of volatilization and gasification to reduce the action reaction can be generated, or the temperature can not be lower than 110 ℃, otherwise, the action reaction can not be carried out.
(C) And finally, a filtering step 12: adsorbing suspended matters of the waste fluorine oil after the physical and chemical reaction, and performing physical reaction treatment by using a settling separation principle to form regenerated fluorine oil; specifically, after the reaction step 11 of (B), the waste fluorine element oil and the chemical agent completely react to present an off-white color, the solution is a suspension, the suspension is adsorbed on the filter element, and the suspension is reduced to the regenerated fluorine element oil with high visibility by physical reaction again, so that the regenerated fluorine element oil is a completely transparent product.
The temperature of the preliminary filtering step 10 and the final filtering step 12 of the step (A) must not exceed 30 ℃, because the preliminary filtering step 10 and the final filtering step 12 of the step (C) cannot bear high temperature, and after the reaction step (B) 11, the temperature of the preliminary filtering step 10 and the final filtering step 12 of the step (A) is reduced to room temperature, which is conducive to physical reaction treatment for solid-liquid separation.
As shown in fig. 2, the method for treating waste fluorine-containing oil further comprises (D) a secondary filtering step 13, wherein D) the secondary filtering step 13 is performed between (B) the reaction step 11 and (C) the final filtering step 12, and if the waste fluorine-containing oil cannot be transparent after passing through (a) the primary filtering step 10, the waste fluorine-containing oil is filtered again by the secondary filtering step 13 to improve the transparency of the waste fluorine-containing oil; specifically, (D) the secondary filtering step 13 is applied to the waste fluorine oil having low visibility and transmittance. If the transmittance and visibility of the waste fluorine-containing oil subjected to the preliminary filtering step 10 of (a) is relatively clear, the secondary filtering step 13 of (D) may be omitted. Wherein the transmittance range is about 85% -99.99%, when the transmittance of the waste fluorine-containing oil filtered by the preliminary filtering step 10 of (A) is lower than the transmittance range, the waste fluorine-containing oil is filtered again by the secondary filtering step 13 of (D).
Example 2:
as shown in fig. 3, a system for treating waste fluorine-containing oil by using the method for treating waste fluorine-containing oil mainly comprises a first filtering device 20, a reaction device 30 and a second filtering device 40.
A first filtering device 20 including an oil inlet 21, a filtering path 22 passing through the oil inlet 21, a plurality of first filtering cartridges 23 positioned on the filtering path 22, and at least one regeneration temporary storage tank 24 connected to one of the first filtering cartridges 23, wherein the plurality of first filtering cartridges 23 are used for filtering the waste fluorine oil impurities passing through the filtering path 22; specifically, the filter paths 22 are connected by pipes. The number of the first filter elements 23 is four, the first filter element 23 is connected to the oil inlet and has an aperture of 5 μm for filtering coarse impurities with a large body diameter, and the apertures of the second to fourth filter elements 23 connected in sequence are 0.1 μm for filtering fine impurities with a small body diameter. The at least one temporary storage tank 24 for regenerated oil is set to two for preventing the oil from filtering too fast to discharge in time. First filter equipment 20 still contains an air exhaust pumping 25 and set up in two regeneration temporary storage grooves 24 with the escape dashpot 26 between the air exhaust pumping 25, air exhaust pumping 25 is arranged in assisting useless fluorine plain oil to flow out in every link is filtered, and escape dashpot 26 is used for preventing useless fluorine plain oil inflow air exhaust pumping 25, and through the assistance of escape dashpot 26, avoids two regeneration temporary storage grooves 24 to overfill, and leads to useless fluorine plain oil to get into air exhaust pumping 25, causes air exhaust pumping 25 to damage.
And the reaction device 30 is connected with the first filtering device 20 and is provided with a reaction tank 31 connected with the two regeneration temporary storage tanks 24, and the reaction tank 31 is used for adding a decoloration adsorption medicament and an alkaline medicament to the filtered waste fluorine-containing oil and controlling the temperature to be in a temperature range above the normal temperature so as to enable the filtered waste fluorine-containing oil to generate a physicochemical reaction.
And the second filtering device 40 is connected with the reaction device 30, and is provided with a second filtering filter element 41 connected with the reaction tank 31 and an oil outlet 42 connected with the second filtering filter element 41, wherein the second filtering filter element 41 is used for adsorbing suspended matters of the waste fluorine oil after the physical and chemical reaction, so that the waste fluorine oil forms regenerated fluorine oil and is discharged from the oil outlet 42.
The above descriptions are the structures of the main components and the configuration description thereof in the embodiments of the present invention. The invention has at least the following effects:
firstly, the cost is reduced, the waste fluorine oil is recycled and regenerated, and the waste fluorine oil can be reused by the industry, so that the purposes of reducing the cost and improving the production and economic benefits are achieved.
And secondly, the environment-friendly benefit is achieved, the waste fluorine oil is repeatedly used, the waste of resources is greatly reduced, and the requirement of environmental pollution is avoided.
In summary, the above embodiments are merely preferred embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalents, improvements, etc. made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (10)

1. A method for treating waste fluorine oil is suitable for being matched with the waste fluorine oil, and is characterized by comprising the following steps:
(A) a primary filtering step: filtering the waste fluorine oil, and removing impurities in the waste fluorine oil through physical reaction treatment of a solid-liquid separation principle;
(B) the reaction steps are as follows: adding a decoloration adsorption agent and an alkaline agent, and controlling the temperature to be in a temperature range above the normal temperature, so that the filtered waste fluorine oil generates a physical and chemical reaction;
(C) and finally, a filtering step: adsorbing suspended matters of the waste fluorine oil after the physical and chemical reaction, and performing physical reaction treatment by using a settling separation principle to form the regenerated fluorine oil.
2. The method for treating waste fluorescein oil as claimed in claim 1, wherein the decolorizing adsorbent agent in the reaction step (B) is selected from one of the following substances: attapulgite, activated carbon, bentonite and zeolite.
3. The method for treating waste fluorescein oil as claimed in claim 1, wherein the alkaline agent in the reaction step (B) is selected from one of the following compounds: calcium hydroxide, calcium carbonate, magnesium carbonate, sodium carbonate.
4. The method for treating waste fluorescein oil as claimed in claim 1, wherein the temperature in the reaction step (B) is in the range of 110-150 ℃.
5. The method for treating waste fluorine-containing oil as claimed in claim 1, further comprising (D) a re-filtration step between the reaction step (B) and the final filtration step (C), wherein if the waste fluorine-containing oil is not transparent to light after the preliminary filtration step (A), the waste fluorine-containing oil is re-filtered by the re-filtration step (D) to increase the transparency of the waste fluorine-containing oil.
6. The method for treating waste fluorescein oil as claimed in claim 1, wherein the dosage of the decolorizing adsorbent agent added in the reaction step (B) is 0.3-0.5g/L, and the dosage of the alkaline agent added is 0.3-0.5 g/L.
7. The method for treating waste fluorescein oil as claimed in claim 1, wherein the temperature of the (A) preliminary filtering step and the (C) final filtering step can not exceed 30 ℃.
8. A waste fluorine oil treatment system using the waste fluorine oil treatment method according to claim 1, comprising:
the first filtering device comprises an oil inlet, a filtering path flowing through the oil inlet, a plurality of first filtering filter elements positioned on the filtering path and at least one regeneration temporary storage tank connected with one of the first filtering filter elements, wherein the first filtering filter elements are used for filtering waste fluorine oil impurities flowing through the filtering path;
the reaction device is connected with the first filtering device and is provided with a reaction tank connected with the at least one regeneration temporary storage tank, and the reaction tank is used for adding a decoloration adsorption medicament and an alkaline medicament to the filtered waste fluorine oil and controlling the temperature to be in a temperature range above the normal temperature so as to enable the filtered waste fluorine oil to generate an action reaction;
and the second filtering device is connected with the reaction device, is provided with a second filtering filter element connected with the reaction tank and an oil outlet connected with the second filtering filter element, and the second filtering filter element is used for adsorbing suspended matters of the waste fluorine oil after the physical and chemical reaction so that the waste fluorine oil forms regenerated fluorine oil and is discharged from the oil outlet.
9. The system of claim 8, wherein the first filtering device further comprises an air pump for assisting the flow of the waste fluorine oil from each stage of filtering, and an escape buffer tank disposed between the at least one regeneration buffer tank and the air pump for preventing the flow of the waste fluorine oil into the air pump.
10. The waste fluorescein oil treatment system as claimed in claim 8, wherein the number of the first filter elements is four, the first filter element is connected with the oil inlet and has a pore size of 5 μm, and the pore size of the second to fourth filter elements connected in sequence is 0.1 μm.
CN201811266447.8A 2018-10-29 2018-10-29 Waste fluoride oil treatment method and system Pending CN111100750A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5966494A (en) * 1982-10-08 1984-04-14 Kanagawaken Purification of waste oil of flon synthetic lubricant
EP0214672A2 (en) * 1985-09-13 1987-03-18 AUSIMONT S.r.l. Process for the purification of oils
EP0224632A1 (en) * 1985-12-06 1987-06-10 Leybold Aktiengesellschaft Process and apparatus for the purification of hydrogen-free fluorized lubricants
US20050194309A1 (en) * 2004-02-26 2005-09-08 Mann & Hummel Gmbh Liquid filter, especially an oil filter for an internal combustion engine
CN101622201A (en) * 2007-02-23 2010-01-06 3M创新有限公司 The purification process that contains the solution of fluorine-based solvent
CN101812349A (en) * 2010-05-11 2010-08-25 上海海都化学科技有限公司 Lubricating oil and grease base oil, and preparation method and applications thereof
CN107603728A (en) * 2017-09-29 2018-01-19 新疆凌志化工有限责任公司 Improve auxiliary agent of final product quality and preparation method thereof after waste lubricating oil regenerates

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5966494A (en) * 1982-10-08 1984-04-14 Kanagawaken Purification of waste oil of flon synthetic lubricant
EP0214672A2 (en) * 1985-09-13 1987-03-18 AUSIMONT S.r.l. Process for the purification of oils
EP0224632A1 (en) * 1985-12-06 1987-06-10 Leybold Aktiengesellschaft Process and apparatus for the purification of hydrogen-free fluorized lubricants
US4756825A (en) * 1985-12-06 1988-07-12 Leybold-Heraeus Gmbh Apparatus for purifying hydrogen-free fluorinated lubricants
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CN101622201A (en) * 2007-02-23 2010-01-06 3M创新有限公司 The purification process that contains the solution of fluorine-based solvent
CN101812349A (en) * 2010-05-11 2010-08-25 上海海都化学科技有限公司 Lubricating oil and grease base oil, and preparation method and applications thereof
CN107603728A (en) * 2017-09-29 2018-01-19 新疆凌志化工有限责任公司 Improve auxiliary agent of final product quality and preparation method thereof after waste lubricating oil regenerates

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
孙发山等: "《基础化学实验》", 30 June 1994, 大连理工大学出版社 *

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Application publication date: 20200505